scholarly journals Development and validation of a rapid turbidimetric assay to determine the potency of norfloxacin in tablets

2015 ◽  
Vol 51 (3) ◽  
pp. 629-635 ◽  
Author(s):  
Lucas Chierentin ◽  
Hérida Regina Nunes Salgado
Keyword(s):  
Inhibitory Effect ◽  
Hplc Method ◽  
Assay Method ◽  
Test Microorganism ◽  
Fluoroquinolone Antibiotics ◽  
Relative Standard ◽  
Significant Difference ◽  
Turbidimetric Assay ◽  
Student’S T ◽  
Development And Validation

Norfloxacin is one of the first commercially available (and most widely used) fluoroquinolone antibiotics. This paper reports the development and validation of a simple, sensitive, accurate and reproducible turbidimetric assay method to quantify norfloxacin in tablets formulations in only 4 hours. The bioassay is based on the inhibitory effect of norfloxacin upon the strain ofStaphylococcus epidermidis ATCC 12228 IAL 2150 used as test microorganism. The assay was performed 3x3 parallel lines like, three tubes for each concentration of reference substance and three tubes for each sample concentration. The results were treated statistically by analysis of variance and were found to be linear (r2 = 0.9999) in the selected range of 25-100 μg mL-1; precise (intra-assay: relative standard deviation (RSD) = 1.33%; inter-assay: RSD = 0.21%), accurate (100.74%) and robust with RSD lower than 4.5%. The student's t-test showed no statistically significant difference between the proposed turbidimetric method and an HPLC method previously validated. However the turbidimetric assay can be used as a valuable alternative methodology for the routine quality control of this medicine, complementary to other physical-chemical methods.

scholarly journals Development and Validation of an Agar Diffusion Assay for Determination of Ceftazidime in Pharmaceutical Preparations

2008 ◽  
Vol 91 (1) ◽  
pp. 59-66 ◽  
Author(s):  
Cleber A Schmidt ◽  
Marcelly Carazzo ◽  
Luciane V Laporta ◽  
Celso F Bittencourt ◽  
Marcos R Santos ◽  
...  
Keyword(s):  
Pharmaceutical Preparations ◽  
Inhibitory Effect ◽  
Intermediate Precision ◽  
Agar Diffusion ◽  
Test Microorganism ◽  
Relative Standard ◽  
Alternative Methodology ◽  
Development And Validation ◽  
Liquid Chromatographic

Abstract Ceftazidime (CFZ) is a broad spectrum parenterallactam antibiotic of the cephalosporin family. This paper reports the development and validation of an agar diffusion microbiological assay using the cylinder-plate method for determination of CFZ in powder for injection. The validation carried out yielded good results in terms of linearity, precision, accuracy, selectivity, and robustness. The assay is based on the inhibitory effect of CFZ upon the strain of Pseudomonas aeruginosa ATCC 27853 used as the test microorganism. The results of the assays were treated statistically by analysis of variance and were found to be linear (correlation coefficient = 0.999998) in the selected range of 8.032.0 g/mL; precise [repeatability: relative standard deviation (RSD) = 1.11; intermediate precision: between-day RSD = 1.37 and between-analyst RSD = 1.41]; and accurate. The selectivity of the bioassay was evaluated by analysis of degraded samples at 50C, and the results were compared with a pharmacopeial liquid chromatographic method at the time 0, 24, and 48 h. The results demonstrated the validity of the proposed bioassay, which allows reliable quantitation of CFZ in pharmaceutical samples and can be used as a useful alternative methodology for CFZ analysis in routine quality control.

scholarly journals Development and In-house Validation of a Microbiological Assay for Determination of Cefepime in Injectable Preparations

2006 ◽  
Vol 89 (5) ◽  
pp. 1367-1372 ◽  
Author(s):  
Marinês J Souza ◽  
Rosecler R Kulmann ◽  
LucÊlia M Silva ◽  
Daniele R Nogueira ◽  
Estevan S Zimmermann ◽  
...  
Keyword(s):  
Micrococcus Luteus ◽  
Inhibitory Effect ◽  
Fourth Generation ◽  
Intermediate Precision ◽  
Test Microorganism ◽  
Relative Standard ◽  
Significant Difference ◽  
Accurate Comparison ◽  
Alternative Methodology

Abstract Cefepime is a new parenteral cephalosporin that has been described as a fourth-generation, broad-spectrum antibiotic. This paper reports the development and in-house validation of an agar diffusion bioassay using a cylinder-plate method for the determination of cefepime in powder for injection. The validation performed yielded good results in terms of linearity, precision, accuracy, and robustness. The assay is based on the inhibitory effect of cefepime upon the strain of Micrococcus luteus ATCC 10240 used as the test microorganism. The results of assays were treated statistically by analysis of variance (ANOVA) and were found to be linear (r = 0.99993) in the selected range of 8.032.0 g/mL; precise [repeatability: relative standard deviation (RSD) = 1.39%, intermediate precision: between-day RSD = 1.77%, and between-analyst RSD = 1.97%] and accurate. Comparison of bioassay and liquid chromatography by ANOVA showed no significant difference between methodologies. The results demonstrated the validity of the proposed bioassay, which is a simple and useful alternative methodology for cefepime determination in routine quality control.

scholarly journals Development and validation of kinetic spectrophotometric method for herbicide bromfenoxim determination

2016 ◽  
Vol 14 (2) ◽  
pp. 115-123
Author(s):  
Emilija Pecev-Marinkovic ◽  
Zora Grahovac ◽  
Snezana Mitic ◽  
Aleksandra Pavlovic ◽  
Ivana Rasic-Misic ◽  
...  
Keyword(s):  
Hydrogen Peroxide ◽  
Detection Limit ◽  
Spectrophotometric Method ◽  
Inhibitory Effect ◽  
Sulfanilic Acid ◽  
Hplc Method ◽  
Optimum Conditions ◽  
Relative Standard ◽  
Kinetic Spectrophotometric ◽  
Development And Validation

A kinetic spectrophotometric method for determining the residues of herbicide bromofenoxim (BrFX) has been developed and validated. The proposed method is based on the inhibitory effect of BrFX on the oxidation of sulfanilic acid (SA) by hydrogen peroxide in the presence of Cu(II) ion, which was monitored at 370 nm. The variables affecting the rate of the reaction were investigated and the optimum conditions were established. BrFX can be measured in the range of 0.041 - 0.46 ?g/ml and 0.46 - 13.86 ?g/ml. The detection limit of the method with 3? criteria is 0.0077 ?g/ml. The relative standard deviations for five replicate determinations of 0.041, 0.24 and 0.46 ?g/ml BrFX are 3.0, 5.32 and 2.85%, respectively. This method can be successfully used to determine BrFX concentration in baby juice samples. The HPLC method is used to verify the results. The results obtained for the same samples by the two methods are quite comparable.

Selective Determination of Entecavir in the Presence of Its Oxidative Degradate by Spectrophotometric and Chromatographic Methods

2021 ◽  
Author(s):  
Heba M El-Sayed ◽  
Laila E Abdel Fattah ◽  
Hisham E Abdellatef ◽  
Maha A Hegazy ◽  
Mai M Abd El-Aziz
Keyword(s):  
High Selectivity ◽  
Oxidative Degradation ◽  
Hplc Method ◽  
Peak Amplitude ◽  
Quality Analysis ◽  
Official Method ◽  
Selective Determination ◽  
Significant Difference ◽  
Development And Validation

Abstract Background Entecavir (ENT) is an antiretroviral agent prescribed for treatment of HBV and HIV. Objective Development and validation of three simple, sensitive, selective, and precise methods for determination of ENT in presence of its oxidative degradation product (ENT deg.). Methods The first method was based on second derivative (D2) spectrophotometry through measuring the peak amplitude of D2 spectra at 293.6 nm. The second one is mean centering of the ratio spectra (MCR), which allowed measuring the peak amplitude at 280.0 nm. While the third method was HPLC; where ENT was separated from ENT deg. using Zobrax C18column and methanol: water (30:70, v/v), pH 3 as a mobile phase. The three developed methods were validated according to ICH guidelines. Results Linearity range of ENT was 5.00–50.00 μg/mL for both D2and MCR. However, higher sensitivity was achieved using HPLC (1.00–50.00 μg/mL). Accuracy of ENT were 100.60%±0.547, 101.55%±1.2071 and 100.61%±1.207 for D2, MCR and HPLC methods, respectively, and precision was within 1.280. Conclusions The developed methods were successfully applied for the determination of ENT in Tecavir® tablets without interference from ENT deg. They showed no significant difference compared with the official method as well as they could be applied in the quality analysis of ENT with high selectivity, accuracy, and precision. Highlights ENT was quantified using two spectrophotometric (D2 and MCR) methods and an HPLC method in presence of ENT deg. The proposed methods were applied to analysis of ENT tablets with high selectivity, sensitivity, and accuracy.

Novel Determination of Anti-Hypertensive Combination; Benidipine Hydrochloride and Nebivolol Hydrochloride by High Performance Chromatographic Method

2021 ◽  
pp. 5433-5438
Author(s):  
V.L.N. Balaji Gupta Tiruveedhi ◽  
Venkateswara Rao Battula ◽  
Kishore Babu Bonige ◽  
Tejeswarudu B.
Keyword(s):  
High Performance ◽  
Degradation Products ◽  
Research Work ◽  
Hplc Method ◽  
Assay Method ◽  
Injection Quantity ◽  
Relative Standard ◽  
Nebivolol Hydrochloride ◽  
Concentration Series

This research work was designed to establish and validate a novel stability indicating RP-HPLC method for the combined determination of Benidipine hydrochloride (BHE) and Nebivolol hydrochloride (NHE) in bulk and tablets, dependent on ICH guidelines.The assay method to analyse BHE and NHE was optimized with isocratic elution using acetonitrile: 0.1M acetate buffer (45:55, pH 5.1), Lichrospher ODS RP-18 column and flow pace of 1 ml/min. Total time for single run was 14 min. The injection quantity was 20μl, and was detected at 249nm. The method was verified on a concentration series of 1.25-10μg/ml (NHE) and 1.0-10μg/ml (BHE) for precision, accuracy and linearity. The LOD values were 0.059µg/ml and 0.028µg/ml for NHE and BHE, respectively. The LOQ values were 0.196µg/ml for NHE and 0.094µg/ml for BHE. The recovery percentages were 98.60-100.11% (BHE) and 98.94-101.50% (NHE) with relative standard deviation 0.250-0.694% (BHE) and 0.183-0.400% (NHE). The method was also observed to be efficient, and was sufficiently specific to measure BHE and NHE in the presence of stress-produced degradation products.

scholarly journals DEVELOPMENT AND STABILITY INDICATING HPLC METHOD FOR DAPAGLIFLOZIN IN API AND PHARMACEUTICAL DOSAGE FORM

2017 ◽  
Vol 9 (5) ◽  
pp. 33 ◽  
Author(s):  
Mitali V. Verma ◽  
Chirag J. Patel ◽  
M. M. Patel
Keyword(s):  
Dosage Form ◽  
Hplc Method ◽  
Assay Method ◽  
Array Detector ◽  
Diode Array Detector ◽  
Hydrogen Phosphate ◽  
Pharmaceutical Dosage Form ◽  
Rp Hplc ◽  
Relative Standard ◽  
Potassium Hydrogen

Objective: To develop precise, accurate and reproducible stability assay method by RP-HPLC for estimation of dapagliflozin in API and pharmaceutical dosage form.Methods: The adequate separation was carried using agilent C18 (4.6 ml (millimeter)*150,5 µm (micromiter), mixture of acetonitrile: di-potassium hydrogen phosphate with pH-6.5 adjusted with OPA (40:60 %v/v) as a mobile phase with the flow rate of 1 ml/min (milliliter/minute) and the effluent was monitored at 222 nm (nanometer) using photo diode array detector. The retention time of dapagliflozin API and dapagliflozin tablet were 3.160 min (minute) and 3.067 min (minute) respectively.Results: Linearity for dapagliflozin was found in the range of 50-150µg/ml (microgram/milliliter) (R2 = 0.99) respectively. The accuracy of the present method was evaluated at 50 %, 100% and 150%. The % recoveries of dapagliflozin API and tablet were found to be in the range of 99.00–99.99 % and 98.50–99.99 % respectively. Precision studies were carried out and the relative standard deviation values were less than two. The method was found to be robust.Conclusion: The proposed method was found to be specific, accurate, precise and robust can be used for estimation of dapagliflozin in API and Pharmaceutical dosage form.

METHOD DEVELOPMENT AND VALIDATION FOR THE SIMULTANEOUS ESTIMATION OF THYMOL AND EUGENOL BY USING RP-HPLC IN PURE AND IN EMULGEL FORMULATION

INDIAN DRUGS ◽  
2021 ◽  
Vol 58 (07) ◽  
pp. 59-65
Author(s):  
Vinita C. Patole ◽  
Shilpa P. Chaudhari ◽  
Keyword(s):  
High Performance ◽  
Method Development ◽  
Limit Of Detection ◽  
Hplc Method ◽  
Simultaneous Estimation ◽  
Limit Of Quantification ◽  
Relative Standard ◽  
Peak Areas ◽  
80 A 20 ◽  
Development And Validation

An attempt was made to develop a simple, selective, rapid and precise high-performance liquid chromatography (HPLC) method for simultaneous estimation of thymol and eugenol. Analysis was performed on a C18 column with the mobile phase consisting of solvent %A (water) and solvent %B (acetonitrile) with the following gradient: 0–1 min, 80 % A, 20 % B; 1–7 min, 40 % A and 60 % B; 7–12 min, 10 % A and 90 % B; and 12–15min, 80 % A and 20 % B at a flow rate of 0.6 mL/min. The compounds were well separated on a Thermo Scientific Hypersil BDS RP C18 column (4.6 mm × 150 mm, dp = 5 µm) and ultraviolet detection at 280 nm. The retention times of eugenol and thymol were 10.5 min and 11.6 min, respectively. Validation of the proposed method was carried out according to the guidelines of the International Council on Harmonization (ICH). The linearity of the method is good for thymol and eugenol over the concentration range of 1–50 ppm, and the r 2 values were 0.9996 for both thymol and eugenol. The calculated limit of detection (LOD) value was 0.5ppm and the limit of quantification (LOQ) value was 1ppm for both the analytes. The intra and interday relative standard deviation (RSD) of the retention time and peak areas was less than 3 %.The established method was appropriate, and the two markers were well resolved, enabling efficient quantitative analysis of thymol and eugenol.

Collaborative Study of Turbidimetric Microbiological Assay of Monensin in Chicken Rations

1977 ◽  
Vol 60 (1) ◽  
pp. 179-182
Author(s):  
H Latham Breunig ◽  
Robert E Scroggs ◽  
Lealon V Tonkinson ◽  
Henry Bikin
Keyword(s):  
Experimental Design ◽  
Collaborative Study ◽  
Microbiological Assay ◽  
Assay Method ◽  
Turbidimetric Method ◽  
Automated Method ◽  
Relative Standard ◽  
Significant Difference ◽  
Feed Form ◽  
Automated Methods

Abstract A turbidimetric microbiological assay method for monensin in chicken rations was submitted in a modified form to 8 collaborating laboratories along with randomized and coded samples. Three laboratories used the manual method and 5 used the automated method. Other factors in the experimental design were ration types (broiler starter, broiler finisher, and pullet grower), feed form (meal vs. pellets), and potency level (90 and 110 g/ton) for one ration. Average recoveries for the ration types over all laboratories and feed forms were 87.7—93.13% of label, while mean recoveries in 2 feed forms were 91.7% for meal and 87.6% for pellets. Average recoveries in the 8 laboratories ranged from 84.6 to 106.64% of label for 90 g/ton rations and 87.1 to 106.6% for 110 g/ton rations. There was no significant difference between the manual and the automated methods. The collaborators’ assays were uniform with respect to within-laboratory variation. Relative standard deviations ranged from 4.51 to 10.76% with a median of 6.04%. Agreement with the plate assay is quite good. The turbidimetric method for monensin has been adopted as official first action.

New and validated RP-HPLC Method for Quantification of Safinamide Mesylate in Presence of Its Basic Degradate, Levodopa and Ondansetron: Application to Human Plasma

2020 ◽  
Vol 58 (9) ◽  
pp. 789-795
Author(s):  
Amira M El-Kosasy ◽  
Lobna A Hussein ◽  
Nesma M Mohamed ◽  
Nahla N Salama
Keyword(s):  
Human Plasma ◽  
High Performance ◽  
Pharmaceutical Preparation ◽  
High Sensitivity ◽  
Reversed Phase ◽  
Hplc Method ◽  
Assay Method ◽  
Ultraviolet Detector ◽  
Rp Hplc ◽  
Significant Difference

Abstract A simple, precise, rapid and accurate reversed-phase high-performance liquid chromatography (RP-HPLC) method was developed and validated for analysis of safinamide mesylate (SAF) in presence of its basic degradate, and co-administered drugs levodopa and ondansetron. The mobile phase consisted of acetonitrile and 20 mM potassium dihyrogen orthophosphate buffer having pH = 5 (40: 60 v/v). Quantification was achieved with ultraviolet detector at 226 nm. The linear range was 0.5–10 μg/mL with mean recovery ± SD of 99.72 ± 1.59. The peak purity of SAF in pharmaceutical preparation spiked with its degradate and co-administered drugs revealed symmetry factor (999.8) within the calculated threshold (>998.1). The suggested method was validated in compliance with the International Conference on Harmonization (ICH) guidelines and statistically compared with the manufacturer HPLC method with no significant difference in terms of accuracy and precision. The assay method was successfully used to estimate SAF in tablets with good percentage recoveries. The high sensitivity (lower than Cmax of the drug 0.65 μg/mL) of the proposed HPLC method enabled the determination of SAF in presence of its basic degradate and co-administered drug, ondansetron in human plasma with acceptable accuracy. The suggested HPLC method could be used in Quality Control (QC) lab for analysis of the studied drug in pharmaceutical preparation.

scholarly journals Development and Validation of a RP-HPLC Method for Quantitative Analysis of Linagliptin in Bulk and Dosage Forms

2018 ◽  
Vol 17 (2) ◽  
pp. 175-182
Author(s):  
Joy Chandra Rajbangshi ◽  
Md Mahbubul Alam ◽  
Md Shahadat Hossain ◽  
Md Samiul Islam ◽  
Abu Shara Shamsur Rouf
Keyword(s):  
Limit Of Detection ◽  
Dosage Forms ◽  
Hplc Method ◽  
Pharmaceutical Dosage Forms ◽  
Rp Hplc ◽  
System Suitability ◽  
Relative Standard ◽  
Limit Of Quantitation ◽  
Precision Limit ◽  
Development And Validation

This research was aimed to establish a versatile, sensitive, rapid and validated RP-HPLC method to analyze linagliptin in bulk as well as in pharmaceutical dosage forms. Liquid chromatography was performed on HPLC system and 20μl of samples were injected into a C18 column (150 x 4.6 mm i.d., 5μm particle size) and the eluents were monitored through a PDA detector at 239 nm. An isocratic method with a flow rate of 1 ml/min was used to elute the compounds with a mobile phase comprised of 70:30 v/v mixture of phosphate buffer (pH 6.8±0.2) and acetonitrile. The retention time of the compound was found to be 2.8 minutes. According to the ICH Q2(R1) guidelines, the method was validated by establishing several analytical parameters such as system suitability, specificity, linearity, accuracy, precision, limit of detection (LOD), limit of quantitation (LOQ), ruggedness and robustness to assay linagliptin. The method showed good linearity (R2 = 0.9981) over the concentration ranges of 40 – 60 μg/ml with a recovery between 99.48% ± 0.38% RSD to 100.22% ± 0.011% RSD, whereas the LOD and LOQ values were 0.05 μg/ml and 0.15 μg/ml, respectively. The relative standard deviation (% RSD) for inter-day and intra-day precision was not more than 2.0%. Hence, the proposed method can be applied accurately for research and routine analysis of linagliptin in bulk as well as different pharmaceutical dosage forms. Dhaka Univ. J. Pharm. Sci. 17(2): 175-182, 2018 (December)

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